黄芪及其蜜炙品的UPLC/Q-TOF-MS分析

Analysis of Astragalus membranaceus and Astragalus fried with honey by UPLC/Q-TOF-MS

目的采用超高效液相色谱与串联四级杆飞行时间质谱仪联用技术(UPLC/Q-TOF-MS)进行黄芪及其蜜炙品的成分分析,并比较蜜炙前后主要成分的变化。方法采用ACQUITY UPLC BEH C18色谱柱,以0.1%(体积分数)甲酸-乙腈-异丙醇体系梯度洗脱,使用ESI离子源,正、负离子模式下采集数据。应用Markerlynx软件进行主成分分析(principal component analysis,PCA),比较药材炮制前后成分变化。结果通过PCA分析,可以很好地区分蜜炙前后的黄芪药材,并鉴定了包括毛蕊异黄酮、芒柄花素、汉黄芪素、3,9-二-O-甲基尼森香豌豆紫檀酚在内的8种蜜炙前后质量分数变化较大的化合物。结论借助UPLC的快速分离和Q-TOF-MS测定的精确分子量信息,结合PCA模式识别方法可以有效地对黄芪药材蜜炙前后化学成分变化进行分析鉴定。

Objective To investigate the change of chemical composition of Astragalus membranaceus and Astragalus fried with honey by ultra-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry（UPLC/Q-TOF-MS）.Methods The chromatographic separation was performed on a ACQUITY UPLC BEH C18 column with a gradient elution of water-acetonitrile-isopropanol.The mass spectrometer equipped with electrospray ionization source was used as detector under the positive and negative ion modes.The difference of Astragalus membranaceus and Astragalus fried with honey were analyzed by principal component analysis（PCA） with Markerlynx software.Results Samples of Astragalus membranaceus and Astragalus fried with honey were apparently classified by PCA.A brief list of 8 differential compounds was presented,including calycosin,formononetin,wogonin and 3,9-di-O-methylnissolin.Conclusion The rapid separation with UPLC and Q-TOF-MS determination of the precise molecular weight information,combined with PCA pattern recognition method can effectively analyze and identify the change of chemical composition of Astragalus membranaceus and Astragalus fried with honey.